IS 1528 (Part 1) : 2010

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Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS
PART 1 DETERMINATION OF PYROMETRIC CONE EQUIVALENT (PCE) OR SOFTENING POINT

( Third Revision )

ICS 81.080

© BIS 2010

B U R EAU O F I N D IAN STAN DAR D S
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002

May 2011

Price Group 2

Refractories Sectional Committee, MTD 15

FOREWORD This Indian Standard (Part 1) (Third Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by the Refractories Sectional Committee had been approved by the Metallurgical Engineering Division Council. This standard was first published in 1953 and subsequently revised in 1974 and 1980. This standard deals with the determination of pyrometric cone equivalent (PCE) or softening point. Other parts in this series are: Part 2 Part 3 Part 4 Part 5 Part 6 Part 7 Part 8 Part 9 Part 10 Part 11 Part 12 Part 13 Part 14 Part 15 Part 16 Part 17 Part 18 Part 19 Part 20 Part 21 Part 22 Determination of refractoriness under load Determination of spalling resistance Determination of cold crushing strength Method for determination of modulus of rupture at ambient temperature of dense and insulating shaped refractory products Determination of permanent linear change after reheating for shaped insulating and dense refractories Methods of sampling and criteria for conformity Determination of apparent porosity Determination and true density Determination of size of refractory bricks Determination of warpage Method for determination of bulk density and true porosity of shaped insulating refractory products Determination of resistance to carbon monoxide Determination of sieve analysis Method for determination of bulk density, apparent porosity and true porosity of dense shaped refractory products Determination of thermal conductivity according to hot-wire method (parallel) Determination of cold crushing strength of shaped insulating refractory products Determination of creep in compression Determination of thermal expansion Determination of modulus of rupture at elevated temperature Determination of thermal conductivity according to hot-wire method (cross-array) Methods for determination of permeability to gases of dense shaped refractory products

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2 : 1960 `Rules for rounding off numerical values ( revised)'. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

IS 1528 (Part 1) : 2010

Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS
PART 1 DETERMINATION OF PYROMETRIC CONE EQUIVALENT (PCE) OR SOFTENING POINT

( Third Revision )

1 SCOPE This standard (Part 1) prescribes the method for determination of pyrometric cone equivalent (PCE) or softening point of refractory materials. 2 REFERENCES The following standards contain provisions, which through reference in this text, constitute provisions of this standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below: IS No. 1528 (Part 7) : 2010 Title Methods of sampling and physical tests for refractory materials: Part 7 Methods of sampling and criteria for conformity (second revision ) Terminology for refractories (first revision )

4.3 Preparation of Samples 4.3.1 Raw Materials Test pieces prepared from raw materials that are subject to considerable modification during reheating shall then be stabilized by heating before their refractoriness is determined. In particular, clays should be calcined at approximately 1 000ºC; after calcination, the test pieces shall comply with the requirements of 4.4.2. 4.3.2 Fired Shapes Take 1 kg of the material. In the case of bricks or shapes, obtain a composite sample from bricks or portions of a number of test pieces taken for other tests, and reduce these fragments in size by means of rolls or jaw crusher adjusted to pass lumps not greater than 5 mm in diameter; take precautions to prevent contamination of the sample with steel particles during crushing or grinding. Reduce the quantity through quartering by different stages of grinding to about 50 g as test sample. Grind the full quantity of the material to pass through 212 micron IS Sieve by suitable grinder or agate mortar. Magnet should be used to separate the iron particles introduced during grinding and crushing operations except in the case of materials, which are themselves magnetic. In order to avoid excessive reduction of the fines, remove them frequently during the process of reduction by throwing the sample on the sieve and continue grinding of coarser particles until all the sample passes through the sieve. Subsequently make specimen as specified in 4.4.1. 4.3.3 For Dry Monolithic Materials Samples of unshaped materials, such as, plastic refractories, ramming materials and refractory cement shall be shaped and fired in a manner appropriate to the material and its condition of use; the firing temperature shall be stated in the test report. 4.3.4 For Mortar make specimen as per dry monolithic

4041 : 2006

3 TERMINOLOGY For the purpose of this standard, the definitions given in IS 4041 shall apply. 4 DETERMINATION OF PYROMETRIC CONE EQUIVALENT (PCE) OR SOFTENING POINT 4.1 Object of Test The object of this test is to determine the softening point of refractory matetials by comparing the test cones prepared from the refractory material under test with standard pyrometric cones. 4.2 Heating Furnace A furnace of the type in which a neutral or oxidizing atmosphere may be maintained shall be preferred.

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IS 1528 (Part 1) : 2010 materials and add the liquid component, if any, in appropriate proportion. Subsequently make specimen as specified in 4.4.1.
NOTE -- At all states, crushing and grinding should be carried out so as to avoid the introduction of extraneous material. At all stages, mixing should be carefully carried out so that the contents of the test pieces are truly representative of the samples.

the help of bonding material. Both the plaque and the bonding material should be of such composition, which will not affect the fusibility of the cones. 4.5.2 Mount the cones with the base embedded approximately 3 mm deep in the plaque, and one of the faces inclined towards the centre of plaque and at an angle of 82° with the horizontal. Arrange the test cones around the outer edge of the plaque with standard cones in between them in the anticipated range, as far as practicable (see Fig. 2). 4.5.3 Place the test plaque with the test pieces and the pyrometric reference cones attached to it in the uniform temperature zone of the furnace. Avoid reducing conditions in the furnace during heating. Take care that the flame does not strike directly against the cones or the cone plaque. Check the furnace at intervals for uniformity of distribution of heat. 4.5.4 Over a period of 1.5 to 2 h, raise the temperature of the furnace to 200°C below the estimated refractoriness temperature of the test material. 4.5.5 Raise the temperature at the rate of 2.5°C/min or at the rate specified by the manufacturer of the cones. Maintain the heating so that at any moment the deviation from the specified temperature rise curve is less than 10°C.

4.4 Preparation of Test Cone 4.4.1 Moulding Mix thoroughly the sample prepared under 4.3.2 and after adding sufficient alkali free dextrin or glue and water, form into test cones in a metal mould, preferably of brass, in the shape of tetrahedron measuring 8 mm on the sides of the base, and 25 mm high (see Fig. 1). 4.4.2 Sintering When dry, subject the test cones, if necessary, to a preliminary burn at a temperature not exceeding 1 000°C for the purpose of sintering them into a firm condition to permit handling. 4.5 Procedure 4.5.1 Mount the test cones and the standard pyrometric cones, the feature of typical standard cones used are reported in Table 1, on a plaque with

FIG. 1 STANDARD PYROMETRIC TEST CONE

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IS 1528 (Part 1) : 2010

FIG. 2 M ETHOD OF MOUNTING TEST CONE AND APPEARANCE AFTER TESTING midway between, report the softening point, for example, Cone Number 31-32. 4.7.3 If the test cone starts bending at an early cone but it is not down until a later cone, report the fact. 4.8 Standard Cone Data The standard pyrometric cone equivalents of standard cones are given in Table 1. 5 SAMPLING CONFORMITY AND CRITERIA FOR

4.6 Softening Point Softening of the cone will be indicated by the top bending over and the tip of the cone touching the plaque surface. 4.7 Report of Results 4.7.1 Report the softening point in terms of the standard pyrometric cone, it being that cone which most nearly corresponds in time of softening with the test cone. 4.7.2 If the test cone softens later than one cone but earlier than the next cone and approximately

The procedure for sampling and the criteria for conformity shall be as laid down in IS 1528 (Part 7).

Table 1 Reference Temperature and Cone Designations (Clauses 4.5.1 and 4.8)
Sl No. Cone Designation Temperature
o

Sl No.

Cone Designation

Temperature
o

C (1) ix) x) xi) xii) xiii) xiv) xv) xvi) (2) ISO 166 ISO 168 ISO 170 ISO 172 ISO 174 ISO 176 ISO 178 ISO 180

C

(1) i) ii) iii) iv) v) vi) vii) viii) NOTES

(2) ISO 150 ISO 152 ISO 154 ISO 156 ISO 158 ISO 160 ISO 162 ISO 164

(3) 1 500 1 520 1 540 1 560 1 580 1 600 1 620 1 640

(3) 1 660 1 680 1 700 1 720 1 740 1 760 1 780 1 800

1 The end point temperatures reported in the table have been obtained from the respective manufacturers' catalogue. 2 Any standard cone is acceptable.

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